CN113340690A - Preparation method of high-purity aluminum gold phase sample - Google Patents
Preparation method of high-purity aluminum gold phase sample Download PDFInfo
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- CN113340690A CN113340690A CN202110587904.9A CN202110587904A CN113340690A CN 113340690 A CN113340690 A CN 113340690A CN 202110587904 A CN202110587904 A CN 202110587904A CN 113340690 A CN113340690 A CN 113340690A
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- -1 aluminum gold Chemical compound 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000005498 polishing Methods 0.000 claims abstract description 72
- 238000000227 grinding Methods 0.000 claims abstract description 64
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 42
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 42
- 230000007797 corrosion Effects 0.000 claims abstract description 22
- 238000005260 corrosion Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000011248 coating agent Substances 0.000 claims abstract description 11
- 238000000576 coating method Methods 0.000 claims abstract description 11
- 238000005070 sampling Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 54
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 24
- 244000137852 Petrea volubilis Species 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 16
- 239000004327 boric acid Substances 0.000 claims description 12
- 238000005520 cutting process Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 8
- 239000010935 stainless steel Substances 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 8
- 238000007517 polishing process Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 125000005619 boric acid group Chemical group 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- 238000000866 electrolytic etching Methods 0.000 claims 1
- 238000002474 experimental method Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 13
- 238000002161 passivation Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000007888 film coating Substances 0.000 description 7
- 238000009501 film coating Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
Abstract
The invention provides a preparation method of a high-purity aluminum-gold phase sample, and relates to the technical field of preparation of aluminum-gold phase samples. The preparation method of the high-purity aluminum gold phase sample provided by the invention comprises the following steps: (1) sampling; (2) marking; (3) grinding; (4) rough polishing; (5) fine polishing; (6) electrolytic polishing; (7) and (4) coating an anode film. According to the technical scheme, electrolytic polishing is adopted in the high-purity aluminum polishing stage, electrolytic corrosion is adopted in the corrosion stage, and compared with the traditional method of preparing a metallographic sample by adopting manual and mechanical polishing, the method is time-saving, efficient, simple and reliable, the prepared metallographic structure is clear and visible, and the experiment reproducibility is high.
Description
Technical Field
The invention relates to the technical field of preparation of aluminum-gold phase samples, in particular to a preparation method of a high-purity aluminum-gold phase sample.
Background
The high-purity aluminum has the properties of low deformation resistance, high conductivity, good plasticity and the like, and is mainly applied to scientific research, electronic industry, chemical industry, manufacture of high-purity alloys, laser materials and other special purposes. High purity aluminum refers to aluminum having an Al content of 99.999% (5N) or more, which has better conductivity, ductility, reflectivity, and corrosion resistance than the original aluminum. In the electronic industry, the method is used for manufacturing high-voltage capacitor aluminum foils, high-performance leads and bonding wires for integrated circuits; in the aerospace industry, high purity aluminum is used for developing and manufacturing plasma sails (the latest power for propelling spacecrafts); in high-speed rail transit, high-speed rail transit vehicles need to prepare high-performance alloy by using high-purity aluminum, and the high-purity aluminum has the characteristics of low magnetic permeability and light specific gravity, so that the high-purity aluminum is widely applied to magnetic suspension materials; in the aspect of optical application, a large number of aluminum reflectors are used in a car lamp reflector, an astronomical telescope and the like in the automobile industry, and high-purity aluminum is also researched to be used as a reflecting surface of a large astronomical telescope abroad. With further understanding and development of the performance of high-purity aluminum, the application prospect of the high-purity aluminum is wider and wider, wherein the grain size and uniformity of the aluminum are one of important influence factors of the material performance. Therefore, the observation of the grain size and uniformity of the high-purity aluminum has high practical value.
In the electrochemical polishing process, the surface of the anode is polarized to generate a passive film, and only the compact passive film can inhibit the crystallographic corrosion of the surface. Because the passivation degree of the convex part and the concave part on the surface of the anode is different, wherein the chemical activity of the convex part is higher, the initially formed passivation film is often incomplete and porous, and the concave part is in a more stable passivation state, the dissolution damage degree of the passivation film of the convex part is higher than that of the concave part, and as a result, the convex part is corroded. The steps are repeated until a stable and compact passivation film layer is obtained, and the electrochemical polishing effect can reach an extreme value. However, the high-purity aluminum is soft, silicon carbide in the sand paper is easily embedded in the process of grinding, and the diamond is easily embedded in the currently selected diamond polishing agent by a mechanical polishing method, so that the metallographic phase is difficult to show after corrosion. Meanwhile, high-purity aluminum is very easy to oxidize to generate an aluminum oxide protective film on the surface, chemical corrosion is difficult to control, and a good metallographic sample is difficult to obtain.
Disclosure of Invention
The invention mainly aims to provide a preparation method of a high-purity aluminum-gold phase sample, and aims to solve the technical problem that a good metallographic sample is difficult to obtain at present.
In order to achieve the purpose, the invention provides a preparation method of a high-purity aluminum-gold phase sample, which is characterized by comprising the following steps:
(1) sampling
Cutting high-purity aluminum as a sample by using water cutting or linear cutting equipment;
(2) marking
Marking the end face and the surface of the metallographic phase to be observed in the sample as a ground face of the sample;
(3) grinding
Grinding the grinding surface of the sample on a grinding disc of a polishing machine, sequentially pressing the grinding surface of the sample on No. 320 water-based abrasive paper, moving the sample along the radial direction and rotating the sample opposite to the rotation direction of the grinding disc to completely eliminate coarse grinding marks and make fine grinding marks consistent;
(4) rough polishing
Rotating the sample treated in the step (2) by 90 degrees, and polishing the sample by using No. 600 water-based sand paper until the surface of the sample is horizontal and has no scratch;
(5) fine polishing
Rotating the sample treated in the step (3) by 90 degrees, polishing the sample by using 1000# water-based sand paper until the surface of the sample is flat and has no scratch, and washing the sample by using water; rotating the sample by 90 degrees, polishing the sample by using No. 2000 water-based abrasive paper until the surface of the sample is flat and has no scratch, and washing the sample by using water;
(6) electrolytic polishing
Taking the sample obtained after the treatment in the step (4) as an anode, taking a stainless steel plate as a cathode, and fully soaking the sample in an electrolytic polishing solution by using an aluminum clip, wherein the electrolytic polishing solution consists of the following components in volume ratio: 70 wt% perchloric acid solution: washing the sample with pure water, spraying absolute ethyl alcohol and drying with a blower by cold air in sequence after the electrolytic polishing is finished;
(7) anode coating film
And (3) taking the sample treated in the step (5) as an anode, taking a stainless steel plate as a cathode, fully soaking the sample in a coating liquid by using an aluminum clamp for electrolytic corrosion, wherein the coating liquid consists of boric acid, hydrofluoric acid and water, and after the electrolytic corrosion is finished, sequentially washing the sample by using pure water, spraying absolute ethyl alcohol and drying by using a blower and cold air to obtain the high-purity aluminum-gold phase sample.
In the traditional manual polishing process, high-purity aluminum is easy to passivate, passivation is caused by the action of metal and oxidizing substances, and a very thin, compact and good-covering-performance passivation film which is firmly adsorbed on the metal surface is generated on the metal surface during action, so that a passivation layer exists on the surface of a sample to influence the observation of a metallographic phase. The method adopts electrolytic polishing in the high-purity aluminum polishing stage, can polish the sample to be bright in a short time, can avoid the situation that a large amount of polishing agent is embedded into the surface of the sample during manual polishing and can avoid the harm caused by rapid oxidation of the sample during manual polishing; the invention uses electrolytic corrosion in the corrosion stage, and can simply and efficiently corrode the aluminum grain boundary. Compared with the existing chemical corrosion method, the metallographic structure prepared by the technical scheme of the invention is clear and visible.
As a preferred embodiment of the preparation method of the high-purity aluminum metallographic specimen, the rotation speed of the grinding process in the step (3) is 300r/min, the grinding time of the end face and the grinding time of the surface are both 5min, and the grinding depth of the end face and the grinding depth of the surface are both 1-2 mm.
The inventor finds that the definition of the high-purity aluminum-gold phase sample structure can be improved by adopting the experimental parameters for grinding through a large amount of experimental researches.
As a preferred embodiment of the preparation method of the high-purity aluminum metallographic specimen, the rotation speed of the rough polishing process in the step (4) is 400r/min, and the grinding time of the end face and the surface is 5 min.
The inventor finds that the prepared high-purity aluminum-gold phase sample has a clearer tissue by adopting the experimental parameters in the rough polishing stage through a large amount of experimental researches.
In the step (5), the rotation speed of the 1000# water-based sand paper is 400r/min, and the grinding time of the end surface and the surface is 5 min; the rotation speed of the grinding by No. 2000 water-based sand paper is 450r/min, and the grinding time of the end face and the surface is 5 min.
As a preferred embodiment of the preparation method of the high-purity aluminum metallographic sample, the voltage of the electrolytic polishing in the step (6) is 20-25V, and the time is 20-40 s.
In a preferred embodiment of the method for preparing a metallographic sample of high purity aluminum according to the present invention, in the coating solution in the step (7), the molar ratio of boric acid, hydrofluoric acid, and water is boric acid: hydrofluoric acid: water 2:9: 20.
As a preferred embodiment of the preparation method of the high-purity aluminum metallographic sample, the voltage of electrolytic corrosion in the step (7) is 10-20V, and the time is 3-8 min.
Compared with the prior art, the invention has the beneficial effects that:
according to the technical scheme, electrolytic polishing is adopted in the high-purity aluminum polishing stage, electrolytic corrosion is adopted in the corrosion stage, and compared with the traditional method of preparing a metallographic sample by adopting manual and mechanical polishing, the method is time-saving, efficient, simple and reliable, the prepared metallographic structure is clear and visible, and the experiment reproducibility is high.
Drawings
FIG. 1 is a metallographic photograph of a high purity aluminum-gold phase sample prepared in example 1 of the present invention;
FIG. 2 is a metallographic photograph of a high purity aluminum-gold phase sample prepared in example 2 of the present invention;
FIG. 3 is a metallographic photograph of a high purity aluminum-gold phase sample prepared in comparative example 1 of the present invention;
FIG. 4 is a metallographic photograph of a high purity aluminum-gold phase sample prepared in comparative example 2 of the present invention.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the following specific examples.
Example 1
The preparation method of the high-purity aluminum gold phase sample of the embodiment comprises the following steps:
(1) sampling
Cutting 15mm by 15mm high-purity aluminum by using a wire cutting device to be used as a sample, wherein the surface needing to be metallographic is required to be flat without obvious concave-convex shape;
(2) marking
Marking an end face (C) and a surface (S) which need to observe a metallographic phase in the sample as a ground surface of the sample;
(3) grinding
Grinding the grinding surface of the sample on a grinding disc of a polishing machine, sequentially pressing the grinding surface of the sample on No. 320 water-based abrasive paper, moving the sample along the radial direction and rotating the sample opposite to the rotation direction of the grinding disc to completely eliminate coarse grinding marks and make fine grinding marks consistent;
(4) rough polishing
Rotating the sample treated in the step (2) by 90 degrees, and polishing the sample by using No. 600 water-based sand paper until the surface of the sample is horizontal and has no scratch;
(5) fine polishing
Rotating the sample treated in the step (3) by 90 degrees, polishing the sample by using 1000# water-based sand paper until the surface of the sample is flat and has no scratch, and washing the sample by using water; rotating the sample by 90 degrees, polishing the sample by using No. 2000 water-based abrasive paper until the surface of the sample is flat and has no scratch, and washing the sample by using water;
(6) electrolytic polishing
Taking the sample obtained after the treatment in the step (4) as an anode, taking a stainless steel plate as a cathode, and fully soaking the sample in an electrolytic polishing solution by using an aluminum clip, wherein the electrolytic polishing solution consists of the following components in volume ratio: 70 wt% perchloric acid solution: washing the sample with pure water, spraying absolute ethyl alcohol and drying with a blower by cold air in sequence after the electrolytic polishing is finished;
(7) anode coating film
Taking the sample treated in the step (5) as an anode, taking a stainless steel plate as a cathode, fully soaking the sample in a film coating solution by using an aluminum clip for electrolytic corrosion, wherein the film coating solution is composed of boric acid, hydrofluoric acid and water, and specifically, the molar ratio of the boric acid to the hydrofluoric acid to the water is boric acid: hydrofluoric acid: forming a mixed solution of 2:9:20 of water to obtain a film coating solution, and washing the sample with pure water, spraying absolute ethyl alcohol and drying the sample with a blower by cold air in sequence after the electrolytic corrosion is finished to obtain a high-purity aluminum-gold phase sample;
wherein the rotating speed in the grinding process in the step (3) is 300r/min, the grinding time of the end face and the grinding time of the surface are both 5min, and the grinding depth of the end face and the grinding depth of the surface are both 1-2 mm;
in the step (4), the rotating speed in the rough polishing process is 400r/min, and the polishing time of the end face and the surface is 5 min;
in the step (5), the rotation speed of polishing with 1000# water-based sand paper is 400r/min, and the polishing time of the end face and the surface is 5 min; the rotational speed of polishing with No. 2000 water-based sand paper is 450r/min, and the polishing time of the end face and the surface is 5 min;
the voltage of the electrolytic polishing in the step (6) is 20-25V, and the time is 20-40 s;
the electrolytic corrosion in the step (7) is carried out at the voltage of 10-20V for 3-8 min.
Effect example 1
The metallographic phase of the high purity aluminum gold phase sample prepared in example 1 was observed, the computer was turned on first, and then the metallographic microscope was turned on. The wiped sample (the high purity aluminum gold phase sample prepared in example 1) was placed on a microscope stage, the microscope objective was switched to a low power lens (5X), the coarse quasi-focal helix was adjusted until the object image was displayed, the fine quasi-focal helix was adjusted until the object image was clear, the polarizer was adjusted, the clearest metallographic photograph was found, and the picture was taken and saved using test software. And then, converting the objective lens into a high power lens, adjusting the coarse focusing screw and the fine focusing screw in sequence until the object image is clear, selecting whether to shoot and store the picture according to actual needs, and marking the grain size on the picture. The metallographic photograph of the high purity aluminum gold phase sample prepared in example 1 is shown in fig. 1.
As can be seen from FIG. 1, the polished surface of the high-purity aluminum is clean and has no scratch, and the gold boundary of the crystal grain is clearly visible, so that the measurement and calculation of the size of the crystal grain are convenient.
Example 2
The preparation method of the high-purity aluminum gold phase sample of the embodiment comprises the following steps:
(1) sampling
Cutting high-purity aluminum with the thickness of 10mm by 15mm by 13mm by using a wire cutting device to be used as a sample, wherein the surface needing to be metallographic is required to be smooth and has no obvious concave-convex shape;
(2) marking
Marking an end face (C) and a surface (S) which need to observe a metallographic phase in the sample as a ground surface of the sample;
(3) grinding
Grinding the grinding surface of the sample on a grinding disc of a polishing machine, sequentially pressing the grinding surface of the sample on No. 320 water-based abrasive paper, moving the sample along the radial direction and rotating the sample opposite to the rotation direction of the grinding disc to completely eliminate coarse grinding marks and make fine grinding marks consistent;
(4) rough polishing
Rotating the sample treated in the step (2) by 90 degrees, and polishing the sample by using No. 600 water-based sand paper until the surface of the sample is horizontal and has no scratch;
(5) fine polishing
Rotating the sample treated in the step (3) by 90 degrees, polishing the sample by using 1000# water-based sand paper until the surface of the sample is flat and has no scratch, and washing the sample by using water; rotating the sample by 90 degrees, polishing the sample by using No. 2000 water-based abrasive paper until the surface of the sample is flat and has no scratch, and washing the sample by using water;
(6) electrolytic polishing
Taking the sample obtained after the treatment in the step (4) as an anode, taking a stainless steel plate as a cathode, and fully soaking the sample in an electrolytic polishing solution by using an aluminum clip, wherein the electrolytic polishing solution consists of the following components in volume ratio: 70 wt% perchloric acid solution: washing the sample with pure water, spraying absolute ethyl alcohol and drying with a blower by cold air in sequence after the electrolytic polishing is finished;
(7) anode coating film
Taking the sample treated in the step (5) as an anode, taking a stainless steel plate as a cathode, fully soaking the sample in a film coating solution by using an aluminum clip for electrolytic corrosion, wherein the film coating solution is composed of boric acid, hydrofluoric acid and water, and specifically, the molar ratio of the boric acid to the hydrofluoric acid to the water is boric acid: hydrofluoric acid: forming a mixed solution of 2:9:20 of water to obtain a film coating solution, and washing the sample with pure water, spraying absolute ethyl alcohol and drying the sample with a blower by cold air in sequence after the electrolytic corrosion is finished to obtain a high-purity aluminum-gold phase sample;
wherein the rotating speed in the grinding process in the step (3) is 300r/min, the grinding time of the end face and the grinding time of the surface are both 5min, and the grinding depth of the end face and the grinding depth of the surface are both 1-2 mm;
in the step (4), the rotating speed in the rough polishing process is 400r/min, and the polishing time of the end face and the surface is 5 min;
in the step (5), the rotation speed of polishing with 1000# water-based sand paper is 400r/min, and the polishing time of the end face and the surface is 5 min; the rotational speed of polishing with No. 2000 water-based sand paper is 450r/min, and the polishing time of the end face and the surface is 5 min;
the voltage of the electrolytic polishing in the step (6) is 20-25V, and the time is 20-40 s;
the electrolytic corrosion in the step (7) is carried out at the voltage of 10-20V for 3-8 min.
Effect example 2
The metallographic phase of the high purity aluminum-gold phase sample prepared in example 2 was observed in the same manner as in effect example 1, and a metallographic photograph of the high purity aluminum-gold phase sample prepared in example 2 is shown in fig. 2.
As can be seen from FIG. 2, the polished surface of the high-purity aluminum is clean and has no scratch, and the gold boundary of the crystal grain is clearly visible, so that the measurement and calculation of the size of the crystal grain are convenient.
Comparative example 1
The comparative example differs from example 1 in that: the process for preparing the high-purity aluminum metallographic specimen does not comprise two processes of electrolytic polishing in the step (6) and anode film coating in the step (7).
The metallographic phase of the high purity aluminum-gold phase sample prepared in comparative example 1 was observed in the same manner as in effect example 1, and the metallographic photograph of the high purity aluminum-gold phase sample prepared in comparative example 1 is shown in fig. 3.
As can be seen from fig. 3, the metallographic structure of the high purity aluminum alloy phase sample prepared in comparative example 1 was blurred, which was not favorable for measurement and calculation of the grain size.
Comparative example 2
The comparative example differs from example 1 in that: the comparative example does not include the step (6) of electropolishing.
The metallographic phase of the high purity aluminum-gold phase sample prepared in comparative example 2 was observed in the same manner as in effect example 1, and the metallographic photograph of the high purity aluminum-gold phase sample prepared in comparative example 2 is shown in fig. 4.
As can be seen from fig. 4, the metallographic structure of the high purity aluminum-gold phase sample prepared in comparative example 2 began to appear but was not clear from example 1, affecting the accuracy of measurement and calculation of the grain size.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (7)
1. The preparation method of the high-purity aluminum-gold phase sample is characterized by comprising the following steps of:
(1) sampling
Cutting high-purity aluminum as a sample by using water cutting or linear cutting equipment;
(2) marking
Marking the end face and the surface of the metallographic phase to be observed in the sample as a ground face of the sample;
(3) grinding
Grinding the grinding surface of the sample on a grinding disc of a polishing machine, sequentially pressing the grinding surface of the sample on No. 320 water-based abrasive paper, moving the sample along the radial direction and rotating the sample opposite to the rotation direction of the grinding disc to completely eliminate coarse grinding marks and make fine grinding marks consistent;
(4) rough polishing
Rotating the sample treated in the step (2) by 90 degrees, and polishing the sample by using No. 600 water-based sand paper until the surface of the sample is horizontal and has no scratch;
(5) fine polishing
Rotating the sample treated in the step (3) by 90 degrees, polishing the sample by using 1000# water-based sand paper until the surface of the sample is flat and has no scratch, and washing the sample by using water; rotating the sample by 90 degrees, polishing the sample by using No. 2000 water-based abrasive paper until the surface of the sample is flat and has no scratch, and washing the sample by using water;
(6) electrolytic polishing
Taking the sample obtained after the treatment in the step (4) as an anode, taking a stainless steel plate as a cathode, and fully soaking the sample in an electrolytic polishing solution by using an aluminum clip, wherein the electrolytic polishing solution consists of the following components in volume ratio: 70 wt% perchloric acid solution: washing the sample with pure water, spraying absolute ethyl alcohol and drying with a blower by cold air in sequence after the electrolytic polishing is finished;
(7) anode coating film
And (3) taking the sample treated in the step (5) as an anode, taking a stainless steel plate as a cathode, fully soaking the sample in a coating liquid by using an aluminum clamp for electrolytic corrosion, wherein the coating liquid consists of boric acid, hydrofluoric acid and water, and after the electrolytic corrosion is finished, sequentially washing the sample by using pure water, spraying absolute ethyl alcohol and drying by using a blower and cold air to obtain the high-purity aluminum-gold phase sample.
2. The method for preparing a sample of a high purity aluminum-gold phase according to claim 1, wherein the rotation speed of the grinding process in the step (3) is 300r/min, the grinding time of the end face and the grinding time of the surface are both 5min, and the grinding depth of the end face and the grinding depth of the surface are both 1-2 mm.
3. The method for preparing a high-purity aluminum-gold phase sample according to claim 1, wherein the rotation speed of the rough polishing process in the step (4) is 400r/min, and the grinding time of the end face and the surface is 5 min.
4. The method for preparing a high-purity aluminum-gold phase sample according to claim 1, wherein in the step (5), the rotation speed of grinding by using No. 1000 water sand paper is 400r/min, and the grinding time of the end face and the surface is 5 min; the rotation speed of the grinding by No. 2000 water-based sand paper is 450r/min, and the grinding time of the end face and the surface is 5 min.
5. The method for preparing a sample of high purity aluminum-gold phase according to claim 1, wherein the voltage for electropolishing in step (6) is 20-25V for 20-40 s.
6. The method for preparing a high-purity aluminum-gold phase sample according to claim 1, wherein in the coating solution of step (7), the molar ratio of boric acid, hydrofluoric acid and water is boric acid: hydrofluoric acid: water 2:9: 20.
7. The method for preparing a sample of high purity aluminum-gold phase according to claim 1, wherein the electrolytic etching in the step (7) is performed at a voltage of 10 to 20V for 3 to 8 min.
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| CN113866200A (en) * | 2021-09-29 | 2021-12-31 | 广西容创新材料产业研究院有限公司 | Preparation method of segregation-method high-purity aluminum EBSD sample |
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